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Characterisation and Study of Compounds by Single Crystal X-ray Diffraction
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Characterisation and Study of Compounds by Single Crystal X-ray Diffraction

A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Crystal Engineering".

Deadline for manuscript submissions: closed (28 October 2023) | Viewed by 21507

Special Issue Editor

Dr. Josefina Perles

E-Mail Website
Guest Editor
Laboratorio de Difracción de Rayos X de Monocristal, SIdI, Universidad Autónoma de Madrid, 28049 Madrid, Spain
Interests: single crystal X-ray diffraction; structure-properties relationship; supramolecular interactions; topological studies
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

After the success of the first volume of the Special Issue “Characterisation and Study of Compounds by Single Crystal X-Ray Diffraction” (https://0-www-mdpi-com.brum.beds.ac.uk/journal/crystals/special_issues/x_ray_diffraction), we launch a second volume due to the continuing interest in this topic.

X-ray diffraction has been widely regarded as the most powerful technique for the structural study of crystalline samples during the last century, as it provides detailed information about the atomic structure of ordered solids regardless of the chemical nature of the sample. Although in the early days, it was mostly applied to mineral samples, the crystallization of natural biological molecules and new synthetic compounds has extended the application of this technique to other disciplines, such as chemistry, biology, materials science or pharmacology.

In particular, single crystal X-ray diffraction (SCXRD) has played a crucial role in the interpretation of the physicochemical properties of many substances, determining with high precision the location of the atoms in the crystal as well as the strength of interatomic bonds and supramolecular interactions. Advances in data collection and treatment have overcome many of the initial limitations, such as small crystal size, twinning or poor crystallinity of the sample, and today, SCXRD is a unique characterization tool for many scientists.

In this Special Issue on the topic of “Characterization and Study of Compounds by Single Crystal X-ray Diffraction”, we want to highlight the importance of this technique in scientific research, alone or in combination with other analytical methods. All contributions involving SCXRD are welcome, and especially those studies in which SCXRD has provided key information to solve experimental problems.

Dr. Josefina Perles
Guest Editor

Manuscript Submission Information

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Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Crystals is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • Crystal structure
  • SCXRD
  • X-ray crystallography
  • Structural study

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Published Papers (17 papers)

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Research

13 pages, 4661 KiB  
Article
Synthesis, Crystal Structure and Photoluminescent Properties of Novel 9-Cyano-Pyrrolo[1,2-a][1,10]Phenanthrolines
by Mihaela Cristea, Mihai Răducă, Sergiu Shova, Constantin Drăghici, Vlad A. Neacșu, Maria Maganu, Loredana Albotă (Barbu), Denisa Dumitrescu and Florea Dumitrascu
Crystals 2024, 14(1), 67; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst14010067 - 07 Jan 2024
Viewed by 986
Abstract
Novel 9-cyano-pyrrolo[1,2-a][1,10]phenanthrolines 6a–d were obtained by an efficient one-pot regioselective reaction between 1,10-phenanthrolinium bromides 2a–d and acrylonitrile as a dipolarophile, in the presence of triethylamine and tetrakis-pyridino-cobalt(II) dichromate (TPCD) as oxidizing agents. The optical properties of the [...] Read more.
Novel 9-cyano-pyrrolo[1,2-a][1,10]phenanthrolines 6a–d were obtained by an efficient one-pot regioselective reaction between 1,10-phenanthrolinium bromides 2a–d and acrylonitrile as a dipolarophile, in the presence of triethylamine and tetrakis-pyridino-cobalt(II) dichromate (TPCD) as oxidizing agents. The optical properties of the compounds were investigated through UV–Vis spectrophotometry and steady-state photoluminescence measurements, while their structures were elucidated by single-crystal X-ray diffraction. The structural characterization revealed that the molecular structures of the four compounds were stabilized by hydrogen bonds and π–π interactions. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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20 pages, 8121 KiB  
Article
Synthesis, Crystal Structure, Hirshfeld Surface Analysis, Energy Framework Calculations, and Halogen Bonding Investigation of Benzene-1,3,5-triyltris((4-chlorophenyl)methanone)
by Hawazen M. Hassanain, Samah Al-Sharif, Huda A. Al-Ghamdi, Layla M. Nahari, Ahlam I. Al-Sulami, Sameera M. Mousally and Khadijah M. Al-Zaydi
Crystals 2024, 14(1), 17; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst14010017 - 24 Dec 2023
Viewed by 993
Abstract
We synthesized 1,3,5-triyltris((4-chlorophenyl)methanone) by a condensation reaction in glacial acetic acid and studied utilizing spectroscopic and analytical techniques such as ultraviolet, infrared, mass, elemental, and nuclear magnetic resonance (NMR) spectroscopy, as well as X-ray crystallography. The effect of chlorine substitution in the 1,3,5-triaroylbenzene [...] Read more.
We synthesized 1,3,5-triyltris((4-chlorophenyl)methanone) by a condensation reaction in glacial acetic acid and studied utilizing spectroscopic and analytical techniques such as ultraviolet, infrared, mass, elemental, and nuclear magnetic resonance (NMR) spectroscopy, as well as X-ray crystallography. The effect of chlorine substitution in the 1,3,5-triaroylbenzene compound in solid-state arrangements was studied. Halogen bonds are detected in the solid-state structures of the titled compound. A dimeric structure is formed due to the presence of two C-Cl···Cl Type I halogen interactions. Additionally, a delocalized Type III C-Cl···π interaction were reported. C-Cl···H hydrogen bonding and π···π interaction were also reported. Hirshfeld surface analysis, 3D fingerprint, the energy framework, and the electro-optic potential were used to evaluate such interactions. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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21 pages, 15462 KiB  
Article
Neutral and Ionic Form of (Benzylthio)Acetic Acid in Novel Aminopyrimidine Based Multi-Component Crystalline Phases
by Justyna Sienkiewicz-Gromiuk and Aleksandra Drzewiecka-Antonik
Crystals 2023, 13(12), 1628; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13121628 - 23 Nov 2023
Viewed by 1037
Abstract
(benzylthio)acetic acid (HBTA) and some aminopyrimidines, namely 2-aminopyrimidine (2-AP), 5-aminopyrimidine (5-AP), 2-amino-4,6-dimethylpyrimidine (2-A-4,6-DMP), and 2,4,6-triaminopyrimidine (2,4,6-TAP), were successfully embodied as structural units into the construction of a total of four novel supramolecular organic frameworks. The received crystalline solids were inspected by single-crystal X-ray [...] Read more.
(benzylthio)acetic acid (HBTA) and some aminopyrimidines, namely 2-aminopyrimidine (2-AP), 5-aminopyrimidine (5-AP), 2-amino-4,6-dimethylpyrimidine (2-A-4,6-DMP), and 2,4,6-triaminopyrimidine (2,4,6-TAP), were successfully embodied as structural units into the construction of a total of four novel supramolecular organic frameworks. The received crystalline solids were inspected by single-crystal X-ray diffraction (SC XRD) in order to obtain insight into the structural and supramolecular facets. The SOFs deriving from 2-AP, 5-AP, and 2-A-4,6-DMP crystallize in the form of co-crystals (1–3), while the one originating from 2,4,6-TAP crystallizes as a salt solvate (4). The SC XRD results indicated the different contents of structural residues present in the asymmetric units of the crystals 1–4 despite using the same molar ratio of molecular co-former components in each case. The molecular structures of co-crystals 1–3 consist of either one neutral residue of each starting component (1 and 3) or one nonionized residue of the aminopyrimidine ingredient and two neutral residues of the acidic component (2). The asymmetric unit of salt solvate 4 is composed of two ionized residues of each co-former (two 2,4,6-TAP+ cations and two BTA− anions) and one MeOH solvent molecule. The most extensive H-bonding network is observed in the crystal structure of salt solvate 4. The relevant molecular ingredients in co-crystals 1–3 are mainly held together by the neutral Ocarboxylic–H···Npyrimidine and Namine–H···Ocarboxylic H-bonds. In the case of aggregate 4, the corresponding ionic residues are predominantly sustained by the charged-assisted Npyrimidinium–H···Ocarboxylate and Namine–H···Ocarboxylate hydrogen interactions. The MeOH solvent, incorporated into the crystal lattice of adduct 4, is also involved in H-bonding by simultaneously serving as the single donor in OMeOH–H···S and the single acceptor in Namine–H···OMeOH H-bonds, which afforded the structural diversity within the 2,4,6-TAP+ cations and BTA− anions. Other weaker sets of additional non-covalent contacts existing in the crystal structures of analyzed conglomerates are involved in the self-assembly, stabilization, and expansion of total supramolecular organic frameworks. The fact of the formation of non-covalent bonded supramolecular organic frameworks in question is also reflected in corresponding results obtained through elemental analysis (EA), Fourier transform infrared spectroscopy (FT–IR), and thermal analysis (TG/DSC). Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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13 pages, 3057 KiB  
Article
The Crystal Structure of Pb10(PO4)6O Revisited: The Evidence of Superstructure
by Sergey V. Krivovichev and Günther Engel
Crystals 2023, 13(9), 1371; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13091371 - 13 Sep 2023
Cited by 5 | Viewed by 1329
Abstract
The crystal structure of Pb10(PO4)6O, the proposed matrix for the potential room-temperature superconductor LK-99, Pb10−xCux(PO4)6O (x = 0.9–1.0), has been reinvestigated via single-crystal X-ray diffraction using crystals prepared by [...] Read more.
The crystal structure of Pb10(PO4)6O, the proposed matrix for the potential room-temperature superconductor LK-99, Pb10−xCux(PO4)6O (x = 0.9–1.0), has been reinvestigated via single-crystal X-ray diffraction using crystals prepared by Merker and Wondratschek (Z. Anorg. Allg. Chem. 1960, 306, 25–29). The crystal structure is trigonal, P3¯, a = 9.8109(6), c = 14.8403(12) Å, V = 1237.06(15), R1 = 0.0413 using 3456 unique observed reflections. The crystal structure of Pb10(PO4)6O is a superstructure with regard to the ‘standard’ P63/m apatite structure type. The doubling of the c parameter is induced through the ordering of the split sites of ‘additional’ O’ atoms within the structure channels running parallel to the c axis and centered at (00z). The O’ atoms form short bonds to the Pb1 atoms, resulting in splitting the Pb1 site into two, Pb1A and Pb1B. The structural distortions are further transmitted to the Pb phosphate framework formed by four Pb2 sites and PO4 groups. The structure data previously reported by Krivovichev and Burns (Z. Kristallogr. 2003, 218, 357–365) may either correspond to the Pb10(PO4)6Ox(OH)2−2x (x ~ 0.4) member of the Pb10(PO4)6O—Pb10(PO4)6(OH)2 solid solution series, or to the high-temperature polymorph of Pb10(PO4)6O (with the phase with doubled c parameter being the low-temperature polymorph). Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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16 pages, 6126 KiB  
Article
Red and Blue-Black Tin Monoxide, SnO: Pitfalls, Challenges, and Helpful Tools in Crystal Structure Determination of Low-Intensity Datasets from Microcrystals
by Hans Reuter
Crystals 2023, 13(8), 1281; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13081281 - 19 Aug 2023
Cited by 1 | Viewed by 918
Abstract
The crystal structures of red and blue-black tin(II) oxide, SnO, have been determined for the first time by single-crystal X-ray diffraction. Blue-black SnO crystallizes in the tetragonal space group P4/nmm, representing a layer structure consisting of the square–pyramidally coordinated tin [...] Read more.
The crystal structures of red and blue-black tin(II) oxide, SnO, have been determined for the first time by single-crystal X-ray diffraction. Blue-black SnO crystallizes in the tetragonal space group P4/nmm, representing a layer structure consisting of the square–pyramidally coordinated tin and slightly distorted tetrahedrally coordinated oxygen atoms, in accordance with previous results. In contrast, red SnO crystallizes in the orthorhombic centrosymmetric space group Pbca rather than in the non-centrosymmetric space group Cmc21, as assumed for a long time. Its layer structure consists of very regular, trigonal–pyramidally coordinated tin atoms as well as trigonal–planar coordinated oxygen atoms. Special care was taken on space group determination, including lattice centering. C-centering could be excluded because of systematic absence violations detected when collecting and processing a primitive triclinic dataset and by generating precession images. In the absence of meaningful extinction conditions resulting from the very small crystal under examination, the structure was initially solved and refined in the triclinic space group P1. Subsequently, the observed atom coordinates were used to reconstruct the actual symmetry skeleton. The various possibilities to identify the correct space group starting from the triclinic solution are demonstrated, and the unique structural features of the crystal structure are visualized. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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17 pages, 4552 KiB  
Article
The High-Pressure Phase Transition in Jamesonite: A Single-Crystal Synchrotron X-ray Diffraction Study
by Paola Comodi, Tonci Balić-Žunić, Maximiliano Fastelli, Michael Hanfland, Ines Collings and Azzurra Zucchini
Crystals 2023, 13(8), 1258; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13081258 - 15 Aug 2023
Viewed by 818
Abstract
The high-pressure behavior of jamesonite (FePb4Sb6S14, a = 4.08(3) Å, b = 19.08(3) Å, c = 15.67(3) Å, β= 91.89°, space group P21/c) has been investigated using in situ HP synchrotron X-ray [...] Read more.
The high-pressure behavior of jamesonite (FePb4Sb6S14, a = 4.08(3) Å, b = 19.08(3) Å, c = 15.67(3) Å, β= 91.89°, space group P21/c) has been investigated using in situ HP synchrotron X-ray single-crystal diffraction up to ~17 GPa with a diamond anvil cell under hydrostatic conditions. Results of the volume isothermal equation of state (EoS), determined by fitting the P-V data with a third-order Birch–Murnaghan (BM) EoS, are V0 = 1207.1(4) Å3, K0 = 36(1) GPa and K’ = 5.7(7). At high pressure, jamesonite undergoes a phase transition to an orthorhombic structure with a Pmcb space group (β-jamesonite). The analysis of β-jamesonite’s compressibility up to 16.6 GPa, studied by fitting the data with a second-order BM-EoS, gives V0 = 1027(2) Å3, K0 = 74(2) GPa. The comparison of the structural refinements at different pressures indicates that Fe, Pb and Sb do not change their coordination number over the whole investigated P range, respectively, 6 for Fe, 7 and 8 for Pb and 5 + 2 for Sb. However, a significant change occurs on the orientation of Sb lone electron pairs upon the phase transition in accordance with the change in symmetry. Furthermore, a discontinuity in the Fe chain evolution at the transition pressure is observed. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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20 pages, 2082 KiB  
Article
Molecular Structures and Intermolecular Hydrogen Bonding of Silylated 2-Aminopyrimidines
by Marcus Herbig, Edwin Kroke and Jörg Wagler
Crystals 2023, 13(7), 990; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13070990 - 21 Jun 2023
Viewed by 783
Abstract
A series of silylated 2-aminopyrimidines Me(4−n)Si(NHpyr)n (Me = methyl, NHpyr = pyrimid-2-ylamino, n = 1, 2, 3, 4), i.e., compounds 1, 2, 3, and 4, respectively, was prepared from a series of the respective [...] Read more.
A series of silylated 2-aminopyrimidines Me(4−n)Si(NHpyr)n (Me = methyl, NHpyr = pyrimid-2-ylamino, n = 1, 2, 3, 4), i.e., compounds 1, 2, 3, and 4, respectively, was prepared from a series of the respective chlorosilanes Me(4−n)SiCln and 2-aminopyrimidine. Triethylamine was used as a sacrificial base. Compounds 1, 2, 3, and 4 are solid at room temperature. They were analyzed using 1H, 13C, 29Si NMR, and Raman spectroscopy, and their molecular structures were confirmed by single-crystal X-ray diffraction analyses. All structures exhibit intramolecular van der Waals contacts between the silicon atom and one nitrogen atom of the pyrimidine moiety. Thus, their Si coordination spheres can be interpreted as [4+n] coordinated capped tetrahedra. Intermolecular hydrogen bonds (N–H···N bridges between the Si-bound amino groups and the non-Si-capping pyrimidine N atoms) are a constant contributor to the solid-state structures of these compounds. Furthermore, compounds 2 and 4 exhibit N–H···N bridges which involve 50% of their Si-capping N atoms as hydrogen bridge acceptors. Consequently, 50% of the non-Si-capping pyrimidine N atoms are stabilized by C–H···N contacts. As a result of a particularly dense network of intermolecular hydrogen bridges, the melting point of Si(NHpyr)4 (compound 4) is higher than 300 °C. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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12 pages, 3420 KiB  
Article
C–H…X (X = F, Cl, Br, I) Versus π-Stacking in the Crystal Packing of Compounds Containing the {M(tpy)X3} Motif
by Catherine E. Housecroft and Edwin C. Constable
Crystals 2023, 13(6), 885; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13060885 - 28 May 2023
Viewed by 933
Abstract
Analysis of the data in the Cambridge Structural Database (CSD) for compounds containing an {M(tpy)X3} motif (tpy = 2,2’:6’,2”-terpyridine, M = any metal, X = F, Cl, Br, I) reveals 17 isostructural mononuclear [M(tpy)X3] compounds crystallizing without lattice solvent; [...] Read more.
Analysis of the data in the Cambridge Structural Database (CSD) for compounds containing an {M(tpy)X3} motif (tpy = 2,2’:6’,2”-terpyridine, M = any metal, X = F, Cl, Br, I) reveals 17 isostructural mononuclear [M(tpy)X3] compounds crystallizing without lattice solvent; both face-to-face π-stacking of pyridine rings and C–H3/H3’…X hydrogen bonding appear to be equally important. Regardless of coordination number (CN = 6, 7 or 8) and nuclearity (mono- or dinuclear), a recurring packing feature in other compounds containing an {M(tpy)X3} unit is the presence of bifurcated Cl…H3/H3’ interactions, complemented in some cases by Cl…H5’/H3” interactions, consistent with the acidic H3, H3’, H5’, and H3” atoms of a coordinated tpy ligand. Octahedral [M(tpy)F3] complexes crystallize as hydrates with strong F…H–OH hydrogen bonding dominating the crystal packing. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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15 pages, 6216 KiB  
Article
M6O4(OH)4 of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from Routine
by Hans Reuter, Dirk Schröder and Kristina Peckskamp
Crystals 2023, 13(5), 739; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13050739 - 27 Apr 2023
Viewed by 1147
Abstract
Single crystals of Sn6O4(OH)4 have been grown over a period of more than a decade in hermetically sealed flasks of various triorganotin(IV)-trihydrides in toluene/N,N-dimethylformamide and those of Pb6O4(OH)4 on [...] Read more.
Single crystals of Sn6O4(OH)4 have been grown over a period of more than a decade in hermetically sealed flasks of various triorganotin(IV)-trihydrides in toluene/N,N-dimethylformamide and those of Pb6O4(OH)4 on a petri dish within some days from the reaction of Pb(ClO4)2 with Sr(OH)2·8H2O. High-resolution X-ray diffraction data of the tetragonally crystallizing compounds have been collected conventionally at 100 K. Crystal structure determinations have been performed in space groups P4/mnc and P4¯21c with different structure models because of a pretended specific systematic extinction condition. Its violation was routinely overseen because of the very low intensities of the respective reflections, an effect reinforced by crystal size. The non-existence of this systematic extinction was experimentally confirmed by studying the datasets in more detail, including the simulation of layer photographs. The importance of additional information obtained from dataset analysis tools and structure validation programs to assess the different structure models is demonstrated. Structures of both molecules are analyzed with respect to the molecules as a whole as well as to their constructive building units: two crystallographic different prototypes of {MO4} coordination polyhedra with a bent seesaw conformation, one μ3-OH- and one μ3-O- group, each trigonal-pyramidally coordinated. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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19 pages, 5744 KiB  
Article
Crystal Structure, Hirshfeld Surface Analysis, and Computational Study of Quinolin-8-yl 4-Chlorobenzoate: Insights from Spectroscopic, Thermal, and Antitumor Properties
by Juan-Carlos Castillo, Diana Becerra and Mario A. Macías
Crystals 2023, 13(4), 694; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13040694 - 18 Apr 2023
Cited by 2 | Viewed by 1474
Abstract
We report the time-efficient synthesis of quinolin-8-yl 4-chlorobenzoate (3) via an O-acylation reaction between 8-hydroxyquinoline (1) and 4-chlorobenzoyl chloride (2) mediated by triethylamine in acetonitrile under heating at 80 °C for 20 min in the Monowave [...] Read more.
We report the time-efficient synthesis of quinolin-8-yl 4-chlorobenzoate (3) via an O-acylation reaction between 8-hydroxyquinoline (1) and 4-chlorobenzoyl chloride (2) mediated by triethylamine in acetonitrile under heating at 80 °C for 20 min in the Monowave 50 reactor. This protocol is distinguished by its short reaction time, operational simplicity, and clean reaction profile. The structure of 3 was fully characterized through a combination of analytical techniques, including NMR, IR, and UV–Vis spectroscopy, MS spectrometry, differential scanning calorimetry (DSC), thermogravimetry (TG), and crystallographic studies. Interestingly, X-ray diffraction analyses of 3 show that the crystal structure is characterized by C-H···N, C-H···O, Cl···π, and π···π interactions. The molecular conformation presents an orthogonal orientation between aromatic rings in the solid state. The calculated interaction energies using the CE-B3LYP model show that dispersion forces act in a higher proportion to build the crystal, which is consistent with the few short hydrogen interactions detected. Electrostatic potential maps suggest the formation of σ-holes over the Cl atoms. Although they can behave as both Lewis acid and base sites, Cl··Cl interactions are absent due to the shallow depth of these σ-holes. Quantum chemical descriptors and global reactivity descriptors were examined using the B3LYP method with the 6-31G(d,p) basis set implemented in CrystalExplorer. Finally, compound 3 exhibited low activity against HOP-92 and EKVX non-Small-cell lung and UO-31 Renal cancer cell lines, with a growth inhibition percentage (GI%) ranging from 6.2% to 18.1%. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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15 pages, 5178 KiB  
Article
Packing Motifs in [M(bpy)2X2] Coordination Compounds (bpy = 2,2′-bipyridine; X = F, Cl, Br, I)
by Edwin C. Constable and Catherine E. Housecroft
Crystals 2023, 13(3), 505; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13030505 - 15 Mar 2023
Cited by 3 | Viewed by 1139
Abstract
Packing motifs within structurally characterized cis-[M(bpy)2X2] (M = any metal, bpy = 2,2′-bipyridine, X = F, Cl, Br, I) coordination compounds have been investigated using data from the Cambridge Structural Database. Compounds fall into two classes: non-solvated cis- [...] Read more.
Packing motifs within structurally characterized cis-[M(bpy)2X2] (M = any metal, bpy = 2,2′-bipyridine, X = F, Cl, Br, I) coordination compounds have been investigated using data from the Cambridge Structural Database. Compounds fall into two classes: non-solvated cis-[M(bpy)2X2] moieties and those with additional lattice molecules (solvent or other molecules). A recurring packing motif is a dimeric unit involving intermolecular face-to-face π-stacking of bpy ligands and CHbpy...X contacts, although in several cases, slippage of the stacked bpy units reduces the effectiveness of the face-to-face interaction leaving the CHbpy...X contacts as the dominant crystal-packing interaction. The prevalence of the dimeric unit versus the assembly of 1D-chains in the solid state is described. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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10 pages, 1919 KiB  
Article
Synthesis, Structure, and Luminescence of a Molecular Europium Tetracyanoplatinate Incorporating 4,5-Diazafluoren-9-One
by Richard E. Sykora
Crystals 2023, 13(2), 317; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13020317 - 14 Feb 2023
Viewed by 1035
Abstract
Eu2(Pt(CN)4)3(H2O)12]·4C11H6N2O·6H2O represents a new member to the lanthanide tetracyanoplatinate family of materials. The synthesis, single-crystal X-ray structure, and photoluminescence properties of this compound are reported [...] Read more.
Eu2(Pt(CN)4)3(H2O)12]·4C11H6N2O·6H2O represents a new member to the lanthanide tetracyanoplatinate family of materials. The synthesis, single-crystal X-ray structure, and photoluminescence properties of this compound are reported herein. The compound contains dimeric [Eu2(Pt(CN)4)3(H2O)12] molecules in which the Eu3+ sites are connected with trans-bridging [Pt(CN)4] 2− anions and co-crystallized along with 4,5-diazafluoren-9-one (dafone) and lattice water. Prominent noncovalent interactions that stabilize the structure include H-bonding as well as short stacking interactions involving the planar tetracyanoplatinate anions in conjunction with the planar dafone molecules. Photoluminescence measurements illustrate that Eu2(Pt(CN)4)3(H2O)12]·4C11H6N2O·6H2O contains multiple emitting states and also displays enhanced Eu3+-based emission due to energy transfer within the compound. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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12 pages, 5427 KiB  
Article
High pO2 Flux Growth and Characterization of NdNiO3 Crystals
by Xiaoli Wang, Shilei Wang, Chao Liu, Chuanyan Fan, Lu Han, Feiyu Li, Tieyan Chang, Yu-Sheng Chen, Shanpeng Wang, Xutang Tao and Junjie Zhang
Crystals 2023, 13(2), 180; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13020180 - 19 Jan 2023
Cited by 1 | Viewed by 1535
Abstract
Single crystals of the perovskite nickelate NdNiO3 with dimensions of up to 50 μm on edge have been successfully grown using the flux method at a temperature of 400 °C and oxygen pressure of 200 bar. The crystals were investigated by a [...] Read more.
Single crystals of the perovskite nickelate NdNiO3 with dimensions of up to 50 μm on edge have been successfully grown using the flux method at a temperature of 400 °C and oxygen pressure of 200 bar. The crystals were investigated by a combination of techniques, including high-resolution synchrotron X-ray single-crystal and powder diffraction and physical property measurements such as magnetic susceptibility and resistivity. Resistivity measurements revealed a metal-insulator transition (MIT) at TMIT~180 K with apparent thermal hysteresis; however, no superlattice peaks or peak splitting below TMIT, which corresponds to a structural transition from Pbnm to P21/n, was observed. The successful growth of NdNiO3 crystals at relatively low temperatures and oxygen pressure provides an alternative approach for preparing single crystals of interesting perovskites such as RNiO3 (R = Sm-Lu) and parent phases of superconducting square planar nickelates. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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17 pages, 3974 KiB  
Article
Dicarboxylic Acid-Based Co-Crystals of Pyridine Derivatives Involving Structure Guiding Unconventional Synthons: Experimental and Theoretical Studies
by Pranay Sharma, Rosa M. Gomila, Antonio Frontera, Miquel Barcelo-Oliver and Manjit K. Bhattacharyya
Crystals 2022, 12(10), 1442; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst12101442 - 12 Oct 2022
Cited by 1 | Viewed by 1447
Abstract
Four co-crystals involving dicarboxylic acids and pyridine derivatives, viz. (ox)0.5(2-CNpy) (1), (adp)(4-CNpy)2 (2), (tp)(4-CNpy)2 (3) and (adp)(3-CNpy)2 (4) (ox = oxalic acid, tp = terephthalic acid, adp = adipic acid, [...] Read more.
Four co-crystals involving dicarboxylic acids and pyridine derivatives, viz. (ox)0.5(2-CNpy) (1), (adp)(4-CNpy)2 (2), (tp)(4-CNpy)2 (3) and (adp)(3-CNpy)2 (4) (ox = oxalic acid, tp = terephthalic acid, adp = adipic acid, CNpy = cyanopyridine), have been synthesized at room temperature in water medium. Crystal-structure analysis of co-crystal 1 reveals the presence of unconventional O···π(oxalic acid)-hole interaction with the C-C bond of ox moiety, along with parallel nitrile–nitrile interactions. The structural topologies of co-crystals 2–4 unfold the presence of antiparallel nitrile–nitrile interactions involving the CNpy moieties. The molecular associations involving the H-bonds and other unconventional contacts among the co-formers of the multicomponent co-crystals are analyzed using density functional theory (DFT) calculations combined with molecular electrostatic potential (MEP) surface, quantum theory of atoms-in-molecules (QTAIM) and noncovalent interaction (NCI) plot computational tools. The computational studies revealed the presence of unconventional O···π-hole interaction in 1 and the H-bonded synthons with π-stacked nitrile contacts involving CNpy moieties in co-crystals 2–4. The energetic features of the noncovalent contacts reveal the crucial roles of the H-bonding synthons and π-stacking interactions in the multicomponent compounds. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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14 pages, 4205 KiB  
Article
To Be or Not to Be a (4,4) Net: Reactions of 4′-{4-(N,N-Diethylaminophenyl)}- and 4′-{4-(N,N-Diphenylaminophenyl)}-3,2′:6′,3″- and 4,2′:6′,4″-Terpyridines with Cobalt(II) Thiocyanate
by Dalila Rocco, Anamarija Nikoletić, Alessandro Prescimone, Edwin C. Constable and Catherine E. Housecroft
Crystals 2022, 12(8), 1136; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst12081136 - 12 Aug 2022
Cited by 2 | Viewed by 1272
Abstract
The ligands 4′-{4-(N,N-diethylaminophenyl)}-3,2′:6′,3″-terpyridine (1) and 4′{4-(N,N-diphenylaminophenyl)}-3,2′:6′,3″-terpyridine (2) were prepared and characterized, including the single crystal structure of 2. Along with their 4,2′:6′,4″-terpyridine isomers, 3 and 4, ligands 1 and 2 were reacted with [...] Read more.
The ligands 4′-{4-(N,N-diethylaminophenyl)}-3,2′:6′,3″-terpyridine (1) and 4′{4-(N,N-diphenylaminophenyl)}-3,2′:6′,3″-terpyridine (2) were prepared and characterized, including the single crystal structure of 2. Along with their 4,2′:6′,4″-terpyridine isomers, 3 and 4, ligands 1 and 2 were reacted with Co(NCS)2 under conditions of crystal growth by layering, using solvent mixtures of MeOH and CHCl3. The single crystal structures of [Co(NCS)2(1)]n·0.8nCHCl3, [Co(NCS)2(2)2(MeOH)2]·3CHCl3, [Co(NCS)2(3)]n·2nCHCl3, and [Co(NCS)2(4)]n were determined. The complexes with 1, 3, and 4 assemble into 2D (4,4) nets with the Co(II) centres as 4-connecting nodes, whereas [Co(NCS)2(2)2(MeOH)2] is a discrete molecular species, illustrating that MeOH can act as a non-innocent solvent. The effects on the structure of changing from the 3,2′:6′,3″-terpyridine (3,2′:6′,3″-tpy) to a 4,2′:6′,4″-tpy metal-binding unit, and of introducing R2N functionalities with different steric demands, are discussed. PXRD of bulk samples of all four products confirmed the single-crystal structures as representative of the bulk materials. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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10 pages, 1985 KiB  
Article
Unexpected Formation of a Silicon-Centered Spirocyclic Oligosiloxane Bearing Eight Pendant Ferrocene Units
by Sonia Bruña, Isabel Cuadrado and Josefina Perles
Crystals 2022, 12(8), 1122; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst12081122 - 11 Aug 2022
Viewed by 1262
Abstract
An intriguing but rare silicon-centered spirocyclic compound, spiro[5.5]octaferrocenylpentasiloxane (4) featuring silicon fused six-membered ferrocenyl-functionalized siloxane rings, has been obtained during the thermally induced transformation of triferrocenylsilane Fc3Si–H (1) into triferrocenylsilanol Fc3Si–OH (2), when [...] Read more.
An intriguing but rare silicon-centered spirocyclic compound, spiro[5.5]octaferrocenylpentasiloxane (4) featuring silicon fused six-membered ferrocenyl-functionalized siloxane rings, has been obtained during the thermally induced transformation of triferrocenylsilane Fc3Si–H (1) into triferrocenylsilanol Fc3Si–OH (2), when N,N-dimethylformamide (DMF) was used as a solvent in the presence of the metal carbonyl Mo(CO)6. The unexpected formation of the maximally ferrocenyl substituted silicon centered spirocyclic 4 involves the obtention, and subsequent condensation, of different ferrocenylsilanol intermediates. Spirocyclic silicate 4 has been characterized using a combination of MALDI-TOF mass spectrometry, elemental analysis, and single crystal X-ray diffraction analysis. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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12 pages, 1993 KiB  
Article
Influence of the Reaction Conditions in the Crystal Structures of Zn(II) and Ni(II) Coordination Compounds with a Dissymmetric Bis(Thiosemicarbazone) Ligand
by Luis Alonso, Rodrigo Burón, Elena López-Torres and Maria Antonia Mendiola
Crystals 2022, 12(3), 310; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst12030310 - 23 Feb 2022
Cited by 4 | Viewed by 1802
Abstract
The new ligand HMeATSM, derived from condensation of 2-3-butanedione with 4-methyl-3-thiosemicarbazide and 2,4-dimethyl-3-thiosemicarbazide, has been synthesized. Its reactivity with nickel(II) and zinc(II) nitrates was explored and the resulting complexes were thoroughly characterized by elemental analysis, conductivity, mass spectrometry, IR, 1H and 13 [...] Read more.
The new ligand HMeATSM, derived from condensation of 2-3-butanedione with 4-methyl-3-thiosemicarbazide and 2,4-dimethyl-3-thiosemicarbazide, has been synthesized. Its reactivity with nickel(II) and zinc(II) nitrates was explored and the resulting complexes were thoroughly characterized by elemental analysis, conductivity, mass spectrometry, IR, 1H and 13C NMR spectroscopies and their structures were confirmed by single-crystal X-ray diffraction. The results showed that the complex [Ni(MeATSM)]NO3 1 is formed under every reaction condition. In contrast, the reaction with zinc(II) nitrate depends on the temperature and the presence of LiOH·H2O, leading to the obtaining of complexes [Zn(MeATSM)(OH2)](NO3) 2 and [Zn(Me2TS)2(OH2)](NO3)2 3. The crystal structures of complexes 1 and 2 show that the dissymmetric ligand acts as a N2S2 tetradentate monoanionic ligand. The structural preferences of the metals also determine the structure of the complexes: whereas nickel(II) is in a square-planar environment, the zinc atom prefers a distorted square-base pyramid geometry imposed by the coordination mode and the planarity of the bis(thiosemicarbazone) ligand. In contrast, in complex 3, containing two bidentate Me2TS ligands, the Zn(II) is in a trigonal bipyramid arrangement. In all the complexes, the nitrate ion is not coordinated to the metal and acts as a counterion. Full article
(This article belongs to the Special Issue Characterisation and Study of Compounds by Single Crystal X-ray Diffraction)
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